KR101560531B1 - Lubricant composition - Google Patents

Abstract

화학식 2

화학식 3

상기 화학식 1, 2 및 3에서,
R¹ 및 R²는 각각 수소원자 또는 직쇄 알킬기 또는 직쇄 알케닐기이고, R¹ 및 R²의 적어도 한쪽은 탄소수 6 내지 12의 직쇄 알킬기 또는 직쇄 알케닐기이며,
R³ 및 R⁴는 각각 수소원자 또는 직쇄 알킬기 또는 직쇄 알케닐기이고, R³ 및 R⁴의 적어도 한쪽은 탄소수 13 내지 18의 직쇄 알킬기 또는 직쇄 알케닐기이며,
R⁵ 및 R⁶은 각각 수소 원자 또는 탄소수 4 내지 30의 분지쇄 알킬기이고, R⁵ 및 R⁶의 적어도 한쪽은 분지쇄 알킬기이다.
윤활유 조성물은 또한 상기 (A) 성분에 유래하는 산가가 0.1 내지 1.0mgKOH/g인 것을 특징으로 한다.The present invention
Lubricating base oils (lubricating base oils), and
(A) 0.01 to 0.5% by mass of at least one selected from acidic phosphate esters represented by the following general formula (1) or (2), (B) 0.01 to 2% by mass of an alkylamine represented by the following general formula Lt; / RTI > and / or reactants.
Formula 1

(2)

(3)

In the above formulas (1), (2) and (3)
R ¹ and R ² are each a hydrogen atom or a straight chain alkyl group or a straight chain alkenyl group, at least one of R ¹ and R ² is a straight chain alkyl group or a straight chain alkenyl group having 6 to 12 carbon atoms,
R ³ and R ⁴ are each a hydrogen atom or a straight chain alkyl group or a straight chain alkenyl group and at least one of R ³ and R ⁴ is a straight chain alkyl group or a straight chain alkenyl group having a carbon number of 13 to 18,
R ⁵ and R ⁶ are each a hydrogen atom or a branched alkyl group having 4 to 30 carbon atoms, and at least one of R ⁵ and R ⁶ is a branched chain alkyl group.
The lubricating oil composition is also characterized in that the acid value derived from the component (A) is 0.1 to 1.0 mg KOH / g.

Description

[0001] LUBRICANT COMPOSITION [0002]

The present invention relates to a lubricating oil composition.

BACKGROUND ART [0002] Lubricants for slip guide surfaces such as machining tables of machine tools are required to have low friction performance, prevention of stick slip, storage stability, corrosion resistance and the like in order to improve machining accuracy. Further, in the case of a machine tool, the lubricating oil for sliding guide surfaces is often mixed with the working fluid of the workpiece. Particularly, when a water-soluble cutting fluid (cutting fluid) is used as the machining fluid, such mixing of the lubricating oil for the sliding guide surfaces causes deterioration of the water-soluble cutting fluid (reduction in cutting performance, acceleration of decay, shortening of mineral oil life, Rise and so on). Therefore, as the performance of the sliding guide surface lubricating oil, lubricating properties such as reduction of the friction coefficient on the sliding guide surface and prevention of stick slippage are excellent, and in consideration of the case where the water-soluble cutting fluid is mixed, And it is demanded not to adversely affect the performance of the water-soluble cutting fluid or lubricating oil for sliding guide surfaces.

As a friction modifier, various extreme pressure agents and oil agents have been used so far. Especially in today's machine tools, there is a growing demand for precision. Phosphoric esters, acidic phosphate esters, carboxylic acids, sulfur compounds, amines, etc. have been used in order to realize friction reduction in a low speed range, [Patent Reference 1, 2, 3, 4]. In addition, attempts have been made to improve stability by neutralizing an acidic phosphate ester with an alkylamine (Patent Document 5).

Patent Document 1: JP-A-8-134488

Patent Document 2: Japanese Laid-Open Patent Publication No. 2001-104973

Patent Document 3: JP-A-2003-171684

Patent Document 4: JP-A No. 2003-430949

Patent Document 5: JP-A-2007-238764

However, in this conventional technique, the load on the environment of the additive is high, and these additives have excellent initial friction performance and positioning performance of the machine tool. However, when the water-soluble cutting fluid is mixed with the lubricant for sliding guide surfaces, The low friction performance is remarkably impaired and the acidic component such as phosphoric acid causes corrosion on the sliding surface of the iron using the iron. This causes deterioration of machining accuracy in the machine tool, The positioning accuracy tends to be deteriorated.

Up to now, attempts have been made to improve stability by neutralizing an acidic phosphate ester with an alkylamine. However, in the combination of conventional additives, it has been difficult to continuously maintain low friction over a long period of time. As a result, an emulsion that continuously maintains excellent friction performance over a long period of time has become necessary.

SUMMARY OF THE INVENTION The present invention has been made in view of the above circumstances and an object of the present invention is to provide a lubricant composition which is excellent in low friction property, positioning property, thermal stability and low temperature storage stability, Lubricating oil composition which is excellent in corrosion resistance, and which is excellent in corrosion resistance.

DISCLOSURE OF THE INVENTION As a result of intensive researches to achieve the above object, the present inventors have found that a lubricant base oil (lubricating base oil) contains a specific mixture of a specific acidic phosphate ester and a specific aliphatic amine and / It has been found that the above problems can be solved by a lubricating oil composition in which the acid value derived from the phosphoric acid ester satisfies a specific condition, and the present invention has been accomplished.

(A) 0.01 to 0.5% by mass of at least one selected from acidic phosphoric acid esters represented by the following general formula (1) or (2), and (B) 0.01 to 2% by mass of an alkylamine represented by the general formula (3) and / or a reactant, and the acid value derived from the component (A) is 0.1 to 1.0 mgKOH / g.

In the above formulas (1), (2) and (3)

R ¹ and R ² may be the same or different and each is a hydrogen atom or a straight chain alkyl group or a straight chain alkenyl group and at least one of R ¹ and R ² is a straight chain alkyl group or a straight chain alkenyl group having 6 to 12 carbon atoms,

R ³ and R ⁴ may be the same or different and each is a hydrogen atom or a straight chain alkyl group or a straight chain alkenyl group and at least one of R ³ and R ⁴ is a straight chain alkyl group or a straight chain alkenyl group having 13 to 18 carbon atoms,

R ⁵ and R ⁶ may be the same or different and each is a hydrogen atom or a branched alkyl group having 4 to 30 carbon atoms, and at least one of R ⁵ and R ⁶ is a branched chain alkyl group.

In the lubricating oil composition of the present invention, it is preferable that the lubricating oil is a lubricating oil base oil having a viscosity index of 105 or more, a saturated hydrocarbon component of 70 mass% or more, and a sulfur content of 0.2 mass% or less.

The nitrogen content of the lubricating base oil is preferably 10 mass ppm or less, and the flash point of the lubricating base oil is preferably 250 deg. C or more.

Further, it is preferable that the lubricating oil composition of the present invention further contains 0.01 to 5% by mass of sulfur compound (C) based on the total amount of the composition.

The lubricating oil composition of the present invention can be used for various applications, but it is preferably used for a machine tool, and particularly preferably used for a sliding guide surface of a machine tool.

According to the lubricating oil composition of the present invention, it is possible to provide a lubricating oil composition which is excellent in low friction property, positional property, thermal stability and low-temperature storage stability and can maintain machining accuracy without significantly deteriorating original low friction property even when a cutting fluid is mixed And furthermore, the corrosion resistance is excellent. Accordingly, the lubricating oil composition of the present invention is extremely useful in terms of stabilization of the operation of the machine tool, longevity, and the like.

1 is a schematic diagram showing a friction coefficient measuring system used in the embodiment.
Explanation of symbols
One… Table, 2 ... A / C servo motor, 3 ... Feed screw, 4 ... Movable jig, 5 ... Load cell, 6 ... Bed, 7 ... Computer, 8 ... Control panel (control panel), 9 ... sinker

Hereinafter, preferred embodiments of the present invention will be described in detail.

There is no particular limitation on the production method of the mineral oil base oil usable in the present invention. For example, the lubricating oil fraction obtained by distilling the crude oil at atmospheric distillation and reduced pressure is subjected to solvent deaeration, solvent extraction, hydrogenolysis, solvent dewaxing, Paraffinic or naphthenic mineral oil obtained by appropriately combining and applying one or more purification means such as contact dewatering, hydrogenation purification, sulfuric acid cleaning, and white soil treatment. The lubricating base oil of the present invention may be blended with oil and / or synthetic oil.

Examples of the fat include fat, lard, soybean oil, rice seed oil, rice bran oil, palm oil, palm oil, palm kernel oil, hydrogenated products thereof and the like.

Examples of the synthetic oil include synthetic hydrocarbon oils such as poly-alpha-olefins (ethylene-propylene copolymer, polybutene, 1-octene oligomer, 1-decene oligomer and hydrides thereof), alkylbenzenes and alkylnaphthalenes . The production method thereof is not particularly limited, but any method can be used as long as it is conventionally produced.

Examples of the synthetic oil other than the synthetic hydrocarbon oil include monoesters (butyl stearate, octyl laurate, etc.), diesters (e.g., ditridecyl glutarate, di-2-ethylhexyl adipate, diisodecyl (Trimellitic acid esters and the like), polyol esters (trimethylolpropane caprylate, trimethylolpropane feralgonate, pentaerythritol, trimethylolpropane trimethacrylate, etc.) 2-ethylhexanoate, pentaerythritol ferrogonate, etc.), polyoxyalkylene glycols, polyphenyl ethers, dialkyl diphenyl ethers, phosphoric acid esters (such as tricresyl phosphate), fluorine compounds Ether, fluorinated polyolefin, etc.), silicone oil, and the like.

In the lubricating oil base oil of the present invention, one kind or two or more kinds of the above-mentioned oil and / or synthetic oil may be combined.

The viscosity of the lubricating base oil used in the present invention is not particularly limited, but the kinematic viscosity at 40 캜 is preferably in the range of 10 to 700 mm 2 / s, more preferably in the range of 15 to 500 mm 2 / s. The content of the lubricating base oil is not particularly limited, but is preferably in the range of 50 to 99.98% by mass based on the total amount of the composition.

As a suitable example of the lubricant base oil used in the present invention, a lubricant base oil (hereinafter referred to as "lubricant base oil according to the present invention") having a viscosity index of 105 or more, a saturated hydrocarbon component of 70 mass% or more, and a sulfur content of 0.2 mass% . Hereinafter, the lubricant base oil according to the present invention will be described in detail.

The lubricant base oil according to the present invention is not particularly limited as long as the viscosity index, the saturated hydrocarbon component and the sulfur content satisfy the above requirements, but preferably the raw oil containing mineral oil and normal paraffin is subjected to hydrogenolysis / hydrogenation isomerization A base oil having a viscosity index of 105 or more, a saturated hydrocarbon component of 70 mass% or more, and a sulfur content of 0.2 mass% or less as a mixture of two or more kinds selected from the group consisting of a lubricating oil base oil (hereinafter also referred to as wax isomerization base oil) .

By setting the viscosity index of the lubricating oil base oil to 105 or more, it becomes possible to obtain a lubricating oil composition capable of more compatible with the oil film forming ability and the fluid resistance reducing ability. When the content of the saturated hydrocarbon is less than 70% by mass, the oxidation stability is markedly lowered, and sludge is easily generated. On the other hand, when the sulfur content exceeds 0.2, the thermal stability is deteriorated and the adverse effect on the friction coefficient is increased, which is not preferable.

In the present invention, the viscosity index means a viscosity index measured in accordance with JIS K 2283-1993. The saturated hydrocarbon component content means a value (unit: mass%) measured in accordance with ASTM D 2007-93.

The nitrogen content of the lubricating oil base oil according to the present invention is preferably 10 mass ppm or less. When the nitrogen content exceeds 10 mass ppm, oxidation stability and thermal stability tend to be lowered. The term "nitrogen component" used in the present invention means nitrogen component measured in accordance with JIS K 2609-1990.

Further, the flash point of the lubricating oil base oil according to the present invention is preferably 250 DEG C or higher. If the flash point is 250 ° C or more, it is not applicable to the dangerous goods of Category 4, "Flammable Liquids" of the Fire Service Act. Classified combustibles are classified as "flammable liquids" and their storage and handling are greatly mitigated as compared with Class 4 dangerous goods. In the present invention, the term "flash point" means a flash point measured in accordance with JIS K 2265.

Further, the lubricating oil composition of the present invention may be blended with a base oil other than the lubricating oil base oil according to the present invention, for example, a lubricant other than the present invention and / or a synthetic oil.

The wax isomerization base oil usable in the present invention is a lubricating oil base oil obtained by subjecting a raw material oil containing normal paraffins described below to hydrogenolysis / hydrogenation isomerization.

As a preferred embodiment of the process for producing a wax isomerization base oil of the present invention, for example, a process for producing a wax isomerization base oil in which the urea duct value of the obtained material to be processed is 4% by mass or less and the viscosity index is 130 or more , And performing a hydrocracking / hydrogenation isomerization so that the NOACK evaporation amount is 15 mass% or less.

Further, the element adduct value in the present invention is measured by the following method. 100 g of a weighed sample oil (wax isomerization base oil) is placed in a round bottom flask, 200 g of urea, 360 ml of toluene and 40 ml of methanol are added, and the mixture is stirred at room temperature for 6 hours. As a result, white granular crystals are produced as a constituent adduct in the reaction liquid. The reaction liquid was filtered with a 1-micron filter to collect the resulting white granular crystals, and the obtained crystals were washed six times with 50 ml of toluene. The recovered white crystals are put into a flask, 300 ml of pure water and 300 ml of toluene are added, and the mixture is stirred at 80 ° C for 1 hour. Separate the aqueous phase with a separatory funnel, and wash the toluene phase three times with 300 ml of pure water. A desiccant (sodium sulfate) was added to the toluene to conduct dehydration treatment, and then toluene was distilled off. The ratio (mass percentage) of the thus obtained element adduct water to the sample oil is defined as the element adduct value.

The NOACK evaporation amount in the present invention means the evaporation loss amount measured in accordance with ASTM D 5800-95.

Another preferred embodiment of the process for producing a lubricating base oil of the present invention is a process for producing a lubricating base oil, which comprises subjecting a raw material oil containing normal paraffin to a process for producing a lubricating base oil, Hydroisomerization / hydrogenation isomerization so that the product of the kinematic viscosity (unit: mm < 2 > / s) at 40 DEG C and the NOACK evaporation amount (unit mass% And a production method of an isomerization base oil.

Further, in the production method of the wax isomerization base oil of the present invention, it is preferable that the raw material oil contains 50 mass% or more of slack wax obtained by solvent removal of the wax isomerization base oil.

The element duct value of the wax isomerization base oil of the present invention is required to be not more than 4% by mass, preferably not more than 3.5% by mass, as described above from the viewpoint of improving the low temperature viscosity property without impairing the viscosity- More preferably 3 mass% or less, and further preferably 2.5 mass% or less. Also, the element duct value of the wax isomerization base oil may be 0 mass%. However, it is preferably not less than 0.1% by mass, more preferably not less than 0.5% by mass, more preferably not less than 0.5% by mass, in view of satisfactory low temperature viscosity characteristics and a wax isomerization base oil having a higher viscosity index, , And particularly preferably 0.8 mass% or more.

The viscosity index of the wax isomerized base oil of the present invention is preferably 105 or more, preferably 110 or more, more preferably 120 or more, still more preferably 130 or more, particularly preferably 100 or more, from the viewpoint of viscosity- Preferably 140 or more.

In producing the wax isomerization base oil of the present invention, a raw material oil containing normal paraffin or wax containing normal paraffin can be used. The raw oil may be either mineral oil or synthetic oil, or a mixture of two or more thereof.

The raw material oil used in the present invention is preferably a wax-containing raw material that boils in the range of lubricating oil specified in ASTM D86 or ASTM D2887. The wax content rate of the raw material oil is preferably 50% by mass or more and 100% by mass or less based on the raw material flow rate. The raw wax content can be measured by analytical methods such as nuclear magnetic resonance spectroscopy (ASTM D5292), correlation analysis (n-d-M) method (ASTM D3238) and solvent method (ASTM D3235).

Examples of the wax-containing raw material include oils derived from a solvent refining method such as raffinate, partial solvent deaerating oil, defatting oil, effluent, reduced pressure gas oil, coca gas oil, slack wax, foots oil, Fischer-Tropsh, wax, and the like, among which slack wax and Fischer-Tropsch wax are preferable.

Slack wax is typically derived from a hydrocarbon feedstock by solvent or propane dewaxing. The slack wax may contain residual oil, but this residual oil can be removed by de-oiling. The foot oil corresponds to the defatted slack wax.

Further, the Fischer Tropsch wax is produced by the so-called Fischer Tropsch synthesis method.

In addition, a commercially available product may be used as a raw material oil containing normal paraffin. Specific examples include Paraflint 80 (hydrogenated Fischer Tropsch wax) and Shell MDS Waxy Raffinate (hydrogenated and partially isomerized middle-flow synthetic waxy raffinate), and the like .

The raw material oil derived from the solvent extraction is obtained by sending a high boiling point oil fraction from the atmospheric distillation to a vacuum distillation apparatus and extracting the distillation oil fraction from the apparatus. The residues from the reduced pressure distillation may be desensitized. In the solvent extraction method, the aromatic component is dissolved into the extracted phase while leaving the more paraffinic component as a raffinate phase. The naphthene are distributed in an extraction phase and a raffinate phase. As the solvent for solvent extraction, phenol, furfural and N-methylpyrrolidone are preferably used. The degree of separation of the extracted phase and the raffinate phase can be controlled by controlling the solvent / oil ratio, the extraction temperature, the method of contacting the effluent and the solvent to be extracted, and the like. As a raw material, a fuel oil hydrocracking apparatus having a higher hydrocracking ability may be used, and a bottom oil obtained from a fuel oil hydrocracking apparatus may be used.

Hydrogenolysis / hydrogenation isomerization is performed on the raw material oil to obtain a wax isomerization base oil of the present invention in such a manner that the value of the element adduct of the obtained product is 4 mass% or less and the viscosity index is 100 or more. can do. The hydrocracking / hydrogenation isomerization process is not particularly limited as long as the element adduct value and viscosity index of the resultant product to be obtained satisfy the above conditions. The preferred hydrogenolysis / hydrogenation isomerization step in the present invention is a hydrogenolysis /

A first step of hydrogenating the raw oil containing normal paraffin using a hydrotreating catalyst,

A second step of subjecting the object to be treated obtained in the first step to hydrogenation-dewaxing using a hydrogenation-dewaxing catalyst and

The third step of hydrogenating and refining the object to be processed obtained by the second step using a hydrogenation purification catalyst

Respectively.

Further, in the conventional hydrocracking / hydrogenation isomerization, in the case where the hydrogenation process is provided at the front stage of the hydrogenation process for the purpose of desulfurization and denitrification for preventing poisoning of the hydrogenation-desalting catalyst have. On the other hand, the first step (hydrotreating step) in the present invention is a step in which a part of the normal paraffin (for example, about 10 mass%, preferably 1 By mass to 10% by mass). Desulfurization and denitrification can be performed in the first step, but the purpose is different from the conventional hydrogenation treatment. Providing such a first step is preferable in ensuring that the value of the element duct of the object to be processed (wax isomerization base oil) obtained after the third step is 4 mass% or less.

Examples of the hydrogenation catalyst used in the first step include catalysts containing Group 6 metals, Group 8-10 metals, and mixtures thereof. Preferred metals include nickel, tungsten, molybdenum, cobalt and mixtures thereof. The hydrogenation catalyst can be used in the form of carrying these metals on a heat-resistant metal oxide support, and usually the metal is present as an oxide or a sulfide on the support. When a mixture of metals is used, the amount of the metal may be present as a bulk metal catalyst of 30 mass% or more based on the whole amount of the catalyst. As the metal oxide carrier, an oxide such as silica, alumina, silica-alumina or titania can be mentioned, and alumina is particularly preferable. Preferred alumina is? -Type or? -Type porous alumina. The supported amount of the metal is preferably in the range of 0.5 to 35% by mass based on the total amount of the catalyst. When a mixture of a Group 9-10 metal and a Group 6 metal is used, either Group 9 or Group 10 metal is present in an amount of 0.1 to 5 mass% based on the total amount of the catalyst, and Group 6 The metal is preferably present in an amount of 5 to 30 mass%. The amount of metal supported may be measured by atomic absorption spectroscopy, inductively coupled plasma emission spectroscopy or by other methods specified in ASTM for each metal.

The acidity of the metal oxide carrier can be controlled by adding additives and controlling the properties of the metal oxide carrier (for example, controlling the amount of silica introduced into the silica-alumina carrier). Examples of additives include halogens, especially fluorine, phosphorus, boron, yttria, alkali metals, alkaline earth metals, rare earth oxides, and magnesia. Co-catalysts such as halogens generally increase the acidity of the metal oxide carrier, while weakly basic additives such as yttria or magnesia tend to weaken the acidity of such a carrier.

Regarding the hydrogenation treatment conditions, the treatment temperature is preferably 150 to 450 占 폚, more preferably 200 to 400 占 폚, the hydrogen partial pressure is preferably 1400 to 20000 kPa, more preferably 2800 to 14000 kPa, The hydrogen / oil ratio is preferably 50 to 1780 m 3 / m 3, more preferably 89 to 890 m 3 / m 3 (LHSV), preferably 0.1 to 10 hr ^-1 , more preferably 0.1 to 5 hr ^-1 . to be. The above conditions are just examples. The conditions for the hydrogenation in the first step for allowing the element adduct value and the viscosity index of the object to be obtained after the third step to satisfy the above-mentioned conditions, respectively, It is preferable to select them appropriately.

The object to be treated after the hydrogenation treatment in the first step may be provided as it is in the second step as it is, but the object to be treated may be subjected to stripping or distillation to separate and remove the gas product from the object (liquid product) Is preferably provided between the first step and the second step. This makes it possible to reduce the nitrogen content and the sulfur content contained in the subject matter to a level that does not affect the long term use of the hydrogenation-desalting catalyst in the second step. The object to be separated and removed by stripping is mainly a gas foreign matter such as hydrogen sulfide and ammonia, and stripping can be carried out by a usual means such as a flash drum, a sorter, and the like.

In the case where the conditions for the hydrogenation treatment in the first step are mild, there is a possibility that the polycyclic aromatic components remaining depending on the raw materials used pass through. These foreign substances are removed by the hydrogenation purification in the third step .

The hydrogenation-desalting catalyst used in the second step may contain any of crystalline or amorphous materials. As the crystalline material, there can be mentioned, for example, a molecular sieve having a 10 or 12-membered ring passage mainly composed of aluminosilicate (zeolite) or silicoaluminophosphate (SAPO). Specific examples of the zeolite include ZSM-22, ZSM-23, ZSM-35, ZSM-48, ZSM-57, ferrierite, ITQ-13, MCM-68 and MCM-71. An example of the aluminophosphate is ECR-42. Examples of the molecular sieve include zeolite beta, and MCM-68. Of these, it is preferable to use one or more kinds selected from ZSM-48, ZSM-22 and ZSM-23, and ZSM-48 is particularly preferable. The molecular sieve is preferably small-sized. Reduction of the hydrogenating dewaxing catalyst may take place at the time of hydrotreating, but the hydrogenating dewaxing catalyst that has been subjected to reduction treatment in advance may be provided in the hydrogenating dewaxing.

Examples of the amorphous material of the hydrogenation-dewaxing catalyst include alumina doped with a Group 3 metal, fluorided alumina, silica-alumina, fluorided silica-alumina, silica-alumina and the like.

A preferred form of the dewaxing catalyst is one having a bifunctional, i.e., a metal hydride component which is at least one Group 6 metal, at least one Group 8-10 metal, or a mixture thereof. Preferred metals are noble metals of group 9-10 such as Pt, Pd or mixtures thereof. The loading amount of these metals is preferably from 0.1 to 30 mass% based on the total amount of the catalyst. Examples of the catalyst preparation and the metal mounting method include an ion exchange method and an impregnation method using a decomposable metal salt.

Further, in the case of using a molecular sieve, it may be combined with a binder material having heat resistance under a hydrogenation dewaxing condition, or even without a binder (magnetic coupling). Examples of the binder material include a combination of two components such as silica, alumina, silica-alumina, silica and other metal oxides such as titania, magnesia, yttria, zirconia and the like, oxides such as silica-alumina-yttria, silica- And inorganic oxides such as a combination of three components. The amount of the molecular sieve in the hydroalcoholization catalyst is preferably 10 to 100 mass%, more preferably 35 to 100 mass%, based on the whole amount of the catalyst. The hydroalcoholization catalyst is formed by spray drying, extrusion, or the like. The hydrodewaxing catalyst can be used in sulfided or unsulfided form, and the sulfided form is preferred.

The hydrogen partial pressure is preferably in the range of 100 to 3000 psig (100 to 3000 psig), more preferably in the range of 1480 to 17339 kPa (200 to 3000 psig) to 2500psig), and the liquid space velocity is preferably from 0.1 to 10hr ^-1, more preferably from 0.1 to 5hr ^-1, hydrogen / suspension ratio is preferably from 45 to 1780㎥ / ㎥ (250 to 10000scf / B), And more preferably 89 to 890 m 3 / m 3 (500 to 5000 scf / B). The hydrogenation-dewatering conditions in the second step for allowing the element adduct value and the viscosity index of the object to be obtained after the third step to satisfy the above-mentioned conditions are the same as those for the raw material, And the like.

The object to be hydrotreated in the second step is provided for the hydrogenation purification in the third step. Hydrogenation purification is a type of mild hydrogenation treatment aiming at saturation of olefins and residual aromatic compounds by hydrogenation in addition to removal of residual heteroatoms and hues. The hydrogenation purification in the third step can be carried out by a dredging process and a cascade method.

The hydrogenation purification catalyst used in the third step is preferably a Group 6 metal, a Group 8-10 metal, or a mixture thereof supported on a metal oxide carrier. Preferable metals include noble metals, particularly platinum, palladium and mixtures thereof. When a mixture of metals is used, the amount of metal may be present as a bulk metal catalyst of 30 mass% or more based on the catalyst. The metal content of the catalyst is preferably 20 mass% or less for the noble metal and 1 mass% or less for the noble metal. As the metal oxide carrier, any of amorphous and crystalline oxides is preferable. Specific examples include low-acid oxides such as silica, alumina, silica-alumina or titania, and alumina is preferable. From the standpoint of saturation of aromatic compounds, it is preferable to use a hydrogenation purification catalyst in which a metal having a relatively strong hydrogenation function is supported on a porous support.

As preferred hydrogenation purification catalysts, mention may be made of mesoporous materials belonging to the M41S class or system of catalysts. The M41S-based catalyst is a mesoporous material having a high silica content, specifically, MCM-41, MCM-48 and MCM-50. Such a hydrogenation purification catalyst has a pore diameter of 15 to 100 ANGSTROM, and MCM-41 is particularly preferable. MCM-41 is an inorganic porous non-layer image having a hexagonal arrangement of pores of the same size. The physical structure of the MCM-41 is the same as a bundle of straw in which the opening of the straw (the cell diameter of the pore) is in the range of 15 to 100 angstroms. MCM-48 has a cubic symmetry, and MCM-50 has a layered structure. MCM-41 can be made with pore openings of different sizes in the mesopore range. The meso porous material may have at least one metal hydrogenation component selected from the group consisting of Group 8, Group 9, and Group 10 metals. As the metal hydrogenation component, a noble metal, particularly, a Group 10 noble metal is preferable, and Pt, Pd, Mixtures are most preferred.

Regarding the conditions of the hydrogenation purification, the temperature is preferably 150 to 350 DEG C, more preferably 180 to 250 DEG C, the voltage is preferably 2859 to 20786 kPa (about 400 to 3000 psig), and the liquid- 0.1 to 5hr ^-1, more preferably from 0.5 to 3hr ^-1, a hydrogen / suspension ratio is preferably from 44.5 to 1780㎥ / ㎥ (250 to 10,000scf / B). The hydrogenation conditions in the third step for allowing the element adduct value and the viscosity index of the object to be obtained after the third step to satisfy the above conditions are the same as the conditions It is preferable to appropriately select it.

Further, with respect to the object to be treated obtained after the third step, if necessary, a predetermined component may be separated and removed by distillation or the like.

In the wax isomerization base oil of the present invention obtained by the following production method, the wax isomerization base oil of the present invention is not particularly limited as long as the urea adduct value and the viscosity index satisfy the above respective conditions, It is desirable to further satisfy the condition.

The content of the saturated component in the wax isomerized base oil of the present invention is 70 mass% or more, preferably 90 mass% or more, more preferably 93 mass% or more, and still more preferably 90 mass% or more, 95% by mass or more. The proportion of the cyclic saturated component in the saturated component is preferably from 0.1 to 50 mass%, more preferably from 0.5 to 40 mass%, still more preferably from 1 to 30 mass%, and particularly preferably from 5 to 20 mass% Mass%. When the content of the saturated component and the proportion of the cyclic saturated component in the saturated component satisfy the above-described conditions, the viscosity-temperature characteristic and the thermal and oxidative stability can be achieved. When the additive is mixed in the wax isomerization base oil , The function of the additive can be expressed at a higher level while sufficiently stably dissolving the additive in the wax isomerization base oil. In addition, by satisfying the above-mentioned conditions, the rubbing characteristics of the wax isomerization base oil itself can be improved, and as a result, the effect of reducing the friction can be improved, and furthermore, the energy An improvement in economy can be achieved.

If the content of the saturated component is less than 70% by mass, the viscosity-temperature characteristics, heat and oxidation stability, and friction characteristics tend to be insufficient. When the ratio of the cyclic saturated component to the saturated component is less than 0.1% by mass, the solubility of the additive becomes insufficient when the additive is added to the wax isomerization base oil, and the effective amount of the additive to be dissolved and retained in the wax isomerization base oil is lowered , There is a tendency that the function of the additive can not be effectively obtained. When the ratio of the cyclic saturated component to the saturated component is more than 50% by mass, the effect of the additive tends to be lowered when the additive is blended in the wax isomerization base oil.

In the present invention, the ratio of the cyclic saturated component to the saturated component is 0.1 to 50 mass%, which is equivalent to 99.9 to 50 mass% of the unsaturated saturated component in the saturated component. Herein, the noncyclic saturated component includes both normal paraffin and isoparaffin. The ratio of the normal paraffin and the isoparaffin in the wax isomerization base oil of the present invention is not particularly limited as long as the value of the element adduct meets the above conditions, but the ratio of isoparaffin is preferably 50 - 99.9 mass%, more preferably 60 to 99.9 mass%, still more preferably 70 to 99.9 mass%, and particularly preferably 80 to 99.9 mass%. When the ratio of isoparaffin occupying the wax isomerization base oil satisfies the above-mentioned condition, the viscosity-temperature characteristic and the thermal / oxidation stability can be further improved. When the additive is added to the wax isomerization base oil, The function of the additive can be expressed at a higher level while stably dissolving.

In the present invention, the content of the saturated component means a value (unit: mass%) measured in accordance with ASTM D 2007-93.

In the present invention, the ratio of the cyclic saturated component and the non-cyclic saturated component to the saturated component is the naphthenic component measured in accordance with ASTM D 2786-91 (measurement object: 1 to 6 ring naphthene, unit: mass %) And an alkane content (unit: mass%).

In the present invention, the ratio of normal paraffin in the wax isomerization base oil is determined by gas chromatography analysis under the following conditions with respect to the saturated component separated and collected by the method described in ASTM D 2007-93, Quot; refers to a value obtained by converting the measured value when the ratio of normal paraffins to the total amount of wax is equalized and quantified based on the total amount of wax isomerization base oil. In the case of identification and quantification, a mixed sample of normal paraffin having 5 to 50 carbon atoms is used as a standard sample. The normal paraffin occupied in the saturated fraction is the total peak area value of the chromatogram (the area value of the peak derived from the diluent is Of the normal paraffin to the normal paraffin).

(Gas chromatographic conditions)

Column: liquid nonpolar column (length 25 cm, inner diameter 0.3 mm, liquid film thickness 0.1 μm)

Temperature raising condition: 50 to 400 占 폚 (temperature raising rate: 10 占 폚 / min)

Carrier gas: helium (linear velocity: 40 cm / min)

Split ratio: 90/1

Sample injection amount: 0.5 μL (amount of sample diluted 20 times with carbon disulfide)

The ratio of isoparaffin in the wax isomerization base oil means a value obtained by converting the difference between the non-cyclic saturated fraction in the saturated fraction and the normal paraffin in the saturated fraction based on the total amount of the wax isomerization base oil.

A similar method can be used for the separation of the saturated components or for the analysis of the components of the cyclic and noncyclic saturated components. For example, the method described in ASTM D 2425-93, the method described in ASTM D 2549-91, the method using high performance liquid chromatography (HPLC), or the method of improving these methods may be mentioned.

In the wax isomerization base oil of the present invention, when the bottom oil fraction obtained from the fuel oil hydrocracking apparatus is used as the raw material, the content of the saturated fraction is 90% by mass or more, and the ratio of the cyclic saturated fraction to the saturated fraction , 30 to 50 mass%, the ratio of the noncyclic saturated component to the saturated component is 50 to 70 mass%, the proportion of isoparaffin in the wax isomerized base oil is 40 to 70 mass%, the viscosity index is 100 to 135, 120 to 130 base oils are obtained but the element duct value satisfies the following conditions, it is possible to obtain the effect of the present invention, especially the excellent low temperature viscosity characteristics of MRV viscosity at -40 캜 of not more than 20000 mPa,, particularly not more than 10000 mPa 을 Lt; RTI ID = 0.0 > Wax < / RTI > Further, in the wax isomerization base oil of the present invention, when a slack wax or a fischer trops wax having a raw material having a high wax content (for example, a normal paraffin content of 50 mass% or more) is used as the raw material, By mass or more, the ratio of the cyclic saturated component to the saturated component is 0.1 to 40% by mass, the ratio of the acyclic saturated component to the saturated component is 60 to 99.9% by mass, the ratio of isoparaffin in the wax isomerized base oil is 60 To 99.9 mass% and a viscosity index of from 100 to 170, preferably from 135 to 160, are obtained. However, by satisfying the following conditions, the effect of the present invention, particularly the MRV viscosity at -40 DEG C, Or less, particularly 7000 mPa · s or less, and a low-temperature viscosity characteristic, can be obtained.

When the refractive index at 20 캜 is n ₂₀ and the kinematic viscosity at 100 캜 is kv 100, the n ₂₀ -0.002 x kv 100 relating to the wax isomerization base oil of the present invention is preferably 1.435 to 1.450, more preferably 1.440 To 1.449, more preferably from 1.442 to 1.448, and still more preferably from 1.444 to 1.447. When n ₂₀ -0.002 x kv 100 is within the above range, excellent viscosity-temperature characteristics and thermal and oxidation stability can be achieved. When the additive is added to the wax isomerization base oil, the additive is sufficiently contained in the wax isomerization base oil The function of the additive can be expressed at a higher level while stably dissolving. By setting n ₂₀ -0.002 x kv 100 within the above range, it is possible to improve the friction characteristics of the wax isomerization base oil itself, and as a result, it is possible to improve the friction reducing effect and further to improve the energy saving.

If n ₂₀ -0.002 x kv 100 exceeds the upper limit value, the viscosity-temperature characteristics, thermal and oxidative stability and friction characteristics become insufficient, and when the additive is added to the wax isomerization base oil, the effect of the additive is lowered There is a tendency. When the additive is added to the wax isomerization base oil, the solubility of the additive becomes insufficient and the effective amount of the additive to be dissolved and held in the wax isomerization base oil is lowered, if n ₂₀ -0.002 x kv 100 is less than the lower limit. There is a tendency that the function of the additive can not be effectively obtained.

In the present invention, the refractive index (n ₂₀ ) at 20 캜 means the refractive index measured at 20 캜 according to ASTM D 1218-92. In the present invention, the kinematic viscosity at 100 캜 (kv 100) means the kinematic viscosity measured at 100 캜 according to JIS K 2283-1993.

The aromatic component in the wax isomerization base oil of the present invention is preferably 5 mass% or less, more preferably 0.05 to 3 mass%, further preferably 0.1 to 1 mass%, based on the whole amount of the wax isomerization base oil %, Particularly preferably 0.1 to 0.5% by mass. If the content of the aromatic component exceeds the above upper limit value, the viscosity-temperature characteristics, thermal and oxidative stability and friction characteristics, and the volatilization-preventing and low-temperature viscosity characteristics tend to be lowered. When the additives are mixed in the wax isomerization base oil The effect of the additive tends to be lowered. The wax isomerization base oil of the present invention may be free of an aromatic component, but the solubility of the additive can be further increased by setting the content of the aromatic component to 0.05% by mass or more.

The term "aromatic content" as used herein means a value measured in accordance with ASTM D 2007-93. In addition to the alkylbenzenes and alkylnaphthalenes, aromatic compounds having an aromatic group such as anthracene, phenanthrene and alkylated compounds thereof, compounds having a benzene ring condensed with four or more rings, pyridines, quinolines, phenols and naphthols Compounds and the like.

The% C _p of the wax isomerization base oil of the present invention is preferably 80 or more, more preferably 82 to 99, still more preferably 85 to 98, particularly preferably 90 to 97. When the% C _p of the wax isomerization base oil is less than 80, the viscosity-temperature characteristics, heat and oxidation stability and friction characteristics tend to be lowered, and when the additives are added to the wax isomerization base oil, There is a tendency. Further, when the% C _p of the wax isomerization base oil exceeds 99, the solubility of the additive tends to be lowered.

The% C _N of the wax isomerization base oil of the present invention is preferably 20 or less, more preferably 15 or less, still more preferably 1 to 12, particularly preferably 3 to 10. If the% C _N of the wax isomerization base oil exceeds 20, the viscosity-temperature characteristics, heat and oxidation stability, and friction characteristics tend to deteriorate. If% C _N is less than 1, the solubility of the additive tends to be lowered.

The% C _A of the wax isomerization base oil of the present invention is preferably 0.7 or less, more preferably 0.6 or less, still more preferably 0.1 to 0.5. If the% C _A of the wax isomerization base oil exceeds 0.7, the viscosity-temperature characteristics, heat and oxidation stability and friction characteristics tend to be lowered. The% C _A of the wax isomerization base oil of the present invention is preferably 0, but when the% C _A is 0.1 or more, the solubility of the additive can be further increased.

Further, the ratio of the% C _P and% C _N of the wax isomerized base oil of the present invention,% C _P /% C _N is more preferably not less than desirable, and 7.5 at least 7, more preferably not less than 8. If the% C _P /% C _N is less than 7, the viscosity-temperature characteristics, heat and oxidation stability and friction characteristics tend to be lowered, and when the additives are added to the wax isomerization base oil, There is a tendency. The% C _P /% C _N is preferably 200 or less, more preferably 100 or less, still more preferably 50 or less, and particularly preferably 25 or less. When% C _P /% C _N is 200 or less, the solubility of the additive can be further increased.

In the present invention,% C _P ,% C _N, and% C _A are the percentages of the number of paraffin carbon atoms relative to the total carbon number, determined by the method according to ASTM D 3238-85 (ndM ring analysis) The percentage of the total number of carbon atoms in the carbon atoms, and the percentage of the total number of carbon atoms in the aromatic carbon atoms. That is, the preferred range of% C _P ,% C _N and% C _A is based on the value obtained by the above method. For example, even a wax isomerization base not containing a naphthene fraction can be obtained by the above- In some cases,% C _N may represent a value exceeding zero.

The iodine value of the wax isomerization base oil of the present invention is preferably 0.5 or less, more preferably 0.3 or less, more preferably 0.15 or less, and even if it is less than 0.01, the effect is small, In view of performance, it is preferably 0.001 or more, and more preferably 0.05 or more. By setting the iodine value of the wax isomerization base oil to 0.5 or less, the thermal and oxidative stability can be remarkably improved. The iodine value referred to in the present invention means the iodine value measured by the indicator titration method of JIS K 0070 "Acid value, saponification value, iodine value, hydroxyl group value and decarboxylation value of a chemical product".

The content of sulfur in the wax isomerization base oil of the present invention depends on the content of sulfur in the raw material. For example, in the case of using a raw material substantially free from sulfur, such as a synthetic wax component obtained by a Fischer Tropsch reaction or the like, a wax isomerization base oil substantially free from sulfur can be obtained. When a raw material containing sulfur such as slack wax obtained in the refining step of the wax isomerization base oil or micro wax obtained in the microfiltration process is used, the sulfur content in the obtained wax isomerization base oil is usually not less than 100 mass ppm . In the wax isomerization base oil of the present invention, the sulfur content is preferably 10 mass ppm or less, more preferably 5 mass ppm or less, and more preferably 3 mass ppm or less, in view of further improvement in thermal and oxidation stability and low- desirable.

In view of cost reduction, it is preferable to use slack wax or the like as a raw material. In that case, the sulfur content in the obtained wax isomerization base oil is preferably 50 mass ppm or less, and more preferably 10 mass ppm or less. In the present invention, the sulfur content means the sulfur content measured in accordance with JIS K 2541-1996.

The content of nitrogen in the wax isomerization base oil of the present invention is 10 ppm or less, preferably 5 mass ppm or less, more preferably 3 mass ppm or less, and further preferably 1 mass ppm or less. If the content of nitrogen is more than 10 mass ppm, the thermal and oxidative stability tends to be lowered. The term "nitrogen component" used in the present invention means nitrogen component measured in accordance with JIS K 2609-1990.

The kinematic viscosity of the wax isomerization base oil of the present invention is preferably 1.5 to 20 mm 2 / s, more preferably 2.0 to 11 mm 2 / s at 100 캜. When the kinematic viscosity at 100 DEG C of the wax isomerized base oil is less than 1.5 mm < 2 > / s, it is not preferable in terms of evaporation loss. Further, when it is desired to obtain a wax isomerization base oil having a kinematic viscosity at 100 캜 exceeding 20 mm 2 / s, the yield is lowered, and even when heavy wax is used as a raw material, it is not preferable to increase the decomposition rate.

In the present invention, it is preferable to use a wax isomerization base oil having a kinematic viscosity at 100 DEG C in the following range by distillation or the like.

A wax isomerization base oil having a kinematic viscosity at 100 DEG C of 4.5 to 20 mm2 / s, more preferably 4.8 to 11 mm2 / s, particularly preferably 5.5 to 8.0 mm2 / s.

The kinematic viscosity at 40 캜 of the wax isomerization base oil of the present invention is preferably 6.0 to 80 mm 2 / s, and more preferably 8.0 to 50 mm 2 / s. In the present invention, it is preferable that the wax isomerized oil having kinematic viscosity at 40 DEG C in the following range is collected by distillation or the like.

A wax isomerization base oil having a kinematic viscosity at 40 캜 of 28 to 50 mm 2 / s, more preferably 29 to 45 mm 2 / s, particularly preferably 30 to 40 mm 2 / s.

In addition, the wax isomerization base oil can satisfy both the viscosity-temperature characteristic and the low-temperature viscosity property at a high level as compared with the conventional lubricant base oil having the same viscosity grade by satisfying the above-mentioned conditions In particular, it has excellent low-temperature viscosity characteristics, and is excellent in anti-volatility, heat and oxidation stability, and lubricity.

Further, the density at 15 ℃ wax isomerized base oil of the invention (ρ _15), the isomerized wax to, depending on the viscosity grade of base oil will be greater than the value of ρ in equation (1), that is preferably in the ρ ₁₅ ≤ρ .

[Equation 1]

ρ = 0.0025 × kv100 + 0.816

In the above equation (1)

kv100 is the kinematic viscosity (mm 2 / s) of the wax isomerization base oil at 100 ° C.

When ρ ₁₅ > ρ, the viscosity-temperature characteristics, thermal and oxidative stability, the volatilization-preventing property and the low-temperature viscosity property tend to be lowered. Further, when the additive is blended in the wax isomerization base oil, The effect tends to be deteriorated.

In the present invention, the density at 15 캜 means the density measured at 15 캜 according to JIS K 2249-1995.

The aniline point (AP (占 폚) of the wax isomerization base oil of the present invention varies depending on the viscosity grade of the wax isomerization base oil, but is preferably not less than the value of A in the following formula (2), that is, AP≥A.

&Quot; (2) "

A = 4.3 x kv 100 + 100

In Equation (2)

kv100 is the kinematic viscosity (mm 2 / s) of the wax isomerization base oil at 100 ° C.

When AP < A is obtained, the viscosity-temperature characteristics, thermal and oxidation stability, the volatilization-preventing property and the low-temperature viscosity property tend to be lowered, and when the additive is added to the wax isomerization base oil, Is lowered.

For example, the AP of the wax isomerization base oil is preferably 125 캜 or higher, and more preferably 128 캜 or higher. The aniline point in the present invention means an aniline point measured in accordance with JIS K 2256-1985.

The NOACK evaporation amount of the wax isomerization base oil is preferably 0% by mass or more, more preferably 1% by mass or more, further preferably 6% by mass or less, further preferably 5% Is not more than 4% by mass. When the NOACK evaporation amount is the lower limit value described above, it tends to be difficult to improve the low temperature viscosity characteristics. Further, when the amount of NOACK evaporation exceeds the upper limit value, the amount of evaporation loss of the wax isomerization becomes large and catalyst poisoning due to the wax isomerization is promoted when the wax isomerization base oil is used for the internal combustion engine lubricating oil or the like.

With respect to the distillation property of the wax isomerization base oil, the boiling point (IBP) thereof is preferably 440 to 480 캜, more preferably 430 to 470 캜, still more preferably 420 to 460 캜. The 10% outflow temperature (T10) is preferably 450 to 510 占 폚, more preferably 460 to 500 占 폚, and still more preferably 460 to 480 占 폚. The 50% outflow point (T50) is preferably 470 to 540 占 폚, more preferably 480 to 530 占 폚, and still more preferably 490 to 520 占 폚. The 90% outflow point (T90) is preferably 470 to 560 占 폚, more preferably 480 to 550 占 폚, and still more preferably 490 to 540 占 폚. Further, the end point (FBP) is preferably 505 to 565 占 폚, more preferably 515 to 555 占 폚, and still more preferably 525 to 565 占 폚. Further, T90-T10 is preferably 35 to 80 占 폚, more preferably 45 to 70 占 폚, and still more preferably 55 to 80 占 폚. Further, the FBP-IBP is preferably 50 to 130 占 폚, more preferably 60 to 120 占 폚, and still more preferably 70 to 110 占 폚. Further, T10-IBP is preferably 5 to 65 占 폚, more preferably 10 to 55 占 폚, and still more preferably 10 to 45 占 폚. Further, the FBP-T90 is preferably 5 to 60 占 폚, more preferably 5 to 50 占 폚, and still more preferably 5 to 40 占 폚.

By setting IBP, T10, T50, T90, FBP, T90-T10, FBP-IBP, T10-IBP and FBP-T90 in the preferred range in the wax isomerization base oil, further improvement in low temperature viscosity, Further reduction is possible. Further, with respect to each of T90-T10, FBP-IBP, T10-IBP and FBP-T90, if the distillation range of these is too narrow, the yield of the wax isomerization base oil is deteriorated,

In the present invention, IBP, T10, T50, T90 and FBP mean the outflow point measured in accordance with ASTM D 2887-97, respectively.

Specifically, the component (A) is a compound represented by the following formulas (1) and (2)

Formula 1

(2)

In the above Formulas 1 and 2,

R ¹ and R ² may be the same or different and each is a hydrogen atom or a straight chain alkyl group or a straight chain alkenyl group and at least one of R ¹ and R ² is a straight chain alkyl group or a straight chain alkenyl group having 6 to 12 carbon atoms,

R ³ and R ⁴ may be the same or different and are each a hydrogen atom or a straight chain alkyl group or a straight chain alkenyl group and at least one of R ³ and R ⁴ is a straight chain alkyl group or a straight chain alkenyl group having 13 to 18 carbon atoms.

Specific examples of the straight-chain alkyl group or straight-chain alkenyl group of R ¹ and R ² include a straight chain hexyl group, a straight chain hexenyl group, a straight chain heptyl group, a straight chain octenyl group, a straight chain octenyl group, a straight chain nonyl group, Specific examples of the alkyl group or the straight chain alkenyl group of R ³ and R ⁴ include straight chain tridecyl, straight chain undecenyl group, straight chain undecenyl group, straight chain dodecyl group, straight chain dodecenyl group, A linear tetradecenyl group, a straight chain tetradecenyl group, a straight chain pentadecenyl group, a straight chain pentadecenyl group, a straight chain hexadecenyl group, a straight chain hexadecenyl group, a straight chain heptadecyl group, a straight chain heptadecenyl group A straight chain octadecenyl group, a straight-chain octadecenyl group, and an oleyl group.

As the component (A) used in the present invention, one of R ¹ and R ² in the above formula (1) or one of R ³ and R ⁴ in the above formula (2) is a hydrogen atom and the other is a linear alkyl group or a straight chain alkenyl group (Phosphoric acid monoesters), and compounds wherein R ¹ and R ² , or both R ³ and R ⁴ are a straight chain alkyl group and / or a straight chain alkenyl group (phosphoric acid diester). In the present invention, one of phosphoric acid monoester or phosphoric acid diester may be used alone, or a mixture of phosphoric acid monoester and phosphoric acid diester may be used. In view of friction characteristics, however, phosphoric acid monoester and phosphoric acid diester It is preferable to use a mixture. When the mixture is used, the mixing ratio of phosphoric acid monoester / phosphoric acid diester is preferably 10/90 to 90/10, more preferably 20/80 to 80/20, and even more preferably 30/70 to 70/30 Is more preferable.

In the lubricating oil composition of the present invention, the content of the component (A) is usually 0.01 to 0.5% by mass based on the total amount of the composition, preferably 0.05% by mass or more, More preferably, it is at least 0.1% by mass. The content of the component (A) is 0.5% by mass or less, preferably 0.4% by mass or less, based on the total amount of the composition, from the viewpoint of excellent corrosion resistance of the obtained lubricating oil composition. The content of the component (A) in the phosphorus element conversion amount varies depending on the molecular weight of the component (A), but is generally from 0.0005 to 0.06 mass%, preferably 0.003 mass% To 0.06% by mass, particularly preferably 0.005 to 0.05% by mass.

In the lubricating oil composition of the present invention, the acid value derived from the component (A) is 0.1 to 1.0 mg / KOH, and if it is less than 0.1, the effect of reducing the friction of the additive is low. It is not preferable that corrosion increases and friction performance can not be maintained for a long period of time.

The component (B) in the present invention is an alkylamine represented by the following general formula (3)

(3)

In Formula 3,

R ⁵ and R ⁶ may be the same or different and each is a hydrogen atom or a branched alkyl group having 4 to 30 carbon atoms, and at least one of R ⁵ and R ⁶ is a branched alkyl group.

In general, the amine represented by the general formula (3) may be any of monoamine, diamine and polyamine having one or more branched alkyl groups having 4 to 30 carbon atoms, preferably 4 to 20 carbon atoms, A monoamine having a branched alkyl group having 2 to 20 carbon atoms is preferable and a secondary amine having a monoamine having two branched alkyl groups having 4 to 20 carbon atoms is preferable. Among these branched alkyl groups, the number of carbon atoms of these branched alkyl groups is more preferably 6 or more, because they are excellent in low temperature storage stability when mixed with the component (A) and low friction performance when a cutting oil is mixed. In terms of solubility in a lubricating base oil, the number of carbon atoms of these branched alkyl groups is preferably 20 or less, more preferably 16 or less, and even more preferably 14 or less.

The preferred branched alkyl group having 4 to 20 carbon atoms is specifically exemplified by isobutyl group, isopentyl group, isohexyl group, isooctyl group, isononyl group, isodecyl group, isonodecyl group, isododecyl group, And branched chain alkyl groups such as a decyl group, an isotetradecyl group, an isopentadecyl group, an isohexadecyl group, an isoheptadecyl group, an isooctadecyl group, an isononadecyl group, and an isoicosyl group.

In the lubricating oil composition of the present invention, the content of the component (B) is usually from 0.01 to 2% by mass based on the total amount of the composition, and from the viewpoint of excellent corrosion resistance when mixed with the component (A) Preferably 0.05 mass% or more, particularly preferably 0.1 mass% or more. The content of the component (B) is preferably 2% by mass or less, more preferably 1.0% by mass or less, and particularly preferably 2% by mass or less, based on the total amount of the composition, from the viewpoint of excellent low temperature storage stability and low friction performance in the presence of cutting oil. Preferably 0.5 mass% or less. The content of the component (B) in terms of the nitrogen element conversion amount varies depending on the molecular weight of the component (B), but is usually 0.0002 to 0.4% by mass, preferably 0.001% To 0.2 mass%, particularly preferably 0.002 to 0.1 mass%.

In the lubricating oil composition of the present invention, the optimum combination of the component (A) and the component (B) includes an acidic phosphate ester having a straight chain alkyl group having 6 to 18 carbon atoms, an amine having a branched chain alkyl group having 4 to 30 carbon atoms, In particular mono-n-octyl sulphate phosphate and / or di-n-octyl sulphate phosphate or monooleyl sulphate phosphate and / or dioleyl acid sulphate and di-2-ethylhexylamine and / or di The combination of tridecylamine is most preferred.

The lubricating oil composition of the present invention is excellent in low friction property and low temperature storage stability by containing the specific lubricant base oil, the component (A) and the component (B), and the initial low friction property is remarkably exhibited even when the cutting fluid is mixed It is possible to maintain the machining accuracy without deteriorating.

The lubricating oil composition of the present invention is preferably added to the lubricating oil composition of the present invention in order to further enhance the performance thereof or to provide the lubricating oil composition for various applications, in particular, a lubricating oil composition for a sliding surface of a machine tool, Other additives may be added.

It is preferable that the lubricating oil composition of the present invention further contains a sulfur compound (C) because the lubricating oil composition of the present invention is excellent in internal performance and can keep the friction coefficient at a lower level and can maintain the processing precision for a long period of time.

Examples of the sulfur compounds (C) include sulfurized oils, sulfurized fatty acids, sulfurized esters, sulfurized olefins, dihydrocarbyl polysulfides, thiadiazole compounds, alkylthiocarbamoyl compounds, thiocarbamate compounds, Thiodipropionate compounds, and the like. These compounds may be used singly or as a mixture of two or more thereof.

Here, the sulfurized oil is obtained by reacting sulfur or a sulfur-containing compound with a fat (lard oil, light oil, vegetable oil, fish oil, etc.). The sulfur content is not particularly limited, but is generally from 5 to 30 mass % Are suitable. Specific examples thereof include sulfurized rods, sulfurized rapeseed oil, sulfated castor oil, sulfurized soybean oil, unsalted rice oil, and mixtures thereof.

Examples of the sulfurized fatty acid include sulfurized oleic acid, and examples of the sulfurized ester include methyl sulfide methyl oleate, octyl sulfated brown rice fatty acid, and mixtures thereof.

As the sulfide olefin, for example, a compound represented by the following formula (4) can be cited:

In Formula 4,

R ⁷ is an alkenyl group having 2 to 15 carbon atoms,

R ⁸ is an alkyl or alkenyl group having 2 to 15 carbon atoms,

a is an integer of 1 to 8;

This compound is obtained by reacting an olefin having 2 to 15 carbon atoms or a 2 to 4-member thereof with a sulfurizing agent such as sulfur or sulfur chloride, and preferred examples of the olefin include propylene, isobutene, diisobutene and the like.

Further, the dihydrocarbyl polysulfide is a compound represented by the following formula (5)

In Formula 5,

R ⁹ and R ¹⁰ are each an alkyl group having 1 to 20 carbon atoms or a cyclic alkyl group, an aryl group having 6 to 20 carbon atoms, an alkylaryl group having 7 to 20 carbon atoms, or an arylalkyl group having 7 to 20 carbon atoms, And,

and b is an integer of 1 to 8.

Here, when R ⁹ and R ¹⁰ are alkyl groups, they are referred to as alkyl sulfides.

Specific examples of R ⁹ and R ¹⁰ in Formula 5 include a methyl group, an ethyl group, a n-propyl group, an isopropyl group, an n-butyl group, an isobutyl group, a sec-butyl group, A cyclohexyl group, a cyclooctyl group, a phenyl group, a naphthyl group, a trityl group, a xylyl group, a benzyl group, a heptyl group, a heptyl group, a heptyl group, a heptyl group, Phenethyl group and the like.

Examples of such dihydrocarbyl polysulfides include dibenzyl polysulfide, various dinonyl polysulfides, various didodecyl polysulfides, various dibutyl polysulfides, various dioctyl polysulfides, diphenyl polysulfides, dicyclohexyl poly Sulfide, a mixture thereof, and the like.

Examples of the thiadiazole compound include 1,3,4-thiadiazole, 1,2,4-thiadiazole compounds, 1,4,5-thiadiazole compounds represented by the following formulas (6), (7) Etc. are preferably used:

In the above formulas (6), (7) and (8)

R ¹¹ and R ¹² each represent a hydrogen atom or a hydrocarbon group having 1 to 20 carbon atoms,

c and d are each an integer of 0 to 8;

Specific examples of such thiadiazole compounds include 2,5-bis (n-hexyldithio) -1,3,4-thiadiazole, 2,5-bis (n-octyldithio) -Thiadiazole, 2,5-bis (n-nonyldithio) -1,3,4-thiadiazole, 2,5-bis (1,1,3,3-tetramethylbutyldithio) -1 , 3,4-thiadiazole, 3,5-bis (n-hexyldithio) -1,2,4-thiadiazole, 3,5-bis (n-octyldithio) -Thiadiazole, 3,5-bis (n-nonyldithio) -1,2,4-thiadiazole, 3,5-bis (1,1,3,3-tetramethylbonalditio) -1 , 2,4-thiadiazole, 4,5-bis (n-hexyldithio) -1,2,3-thiadiazole, 4,5-bis (n-octyldithio) (Thiadiazole), 4,5-bis (n-nonyldithio) -1,2,3-thiadiazole, 4,5-bis (1,1,3,3-tetramethylbutyldithio) -1 , 2,3-thiadiazole, and mixtures thereof.

As the alkylthiocarbamoyl compound, for example, there can be mentioned a compound represented by the following formula (9)

In the above formula (9)

R ¹³ to R ¹⁶ are each an alkyl group having 1 to 20 carbon atoms,

e is an integer of 1 to 8;

Specific examples of such alkylthiocarbamoyl compounds include bis (dimethylthiocarbamoyl) monosulfide, bis (dibutylthiocarbamoyl) monosulfide, bis (dimethylthiocarbamoyl) disulfide, bis ) Disulfide, bis (diamylthiocarbamoyl) disulfide, bis (dioctylthiocarbamoyl) disulfide, and mixtures thereof.

The alkylthiocarbamate compound includes, for example, a compound represented by the following formula (10): &lt; EMI ID =

In Formula 10,

R ¹³ to R ¹⁶ are each an alkyl group having 1 to 20 carbon atoms,

And R &lt; ¹⁷ &gt; is an alkyl group having 1 to 10 carbon atoms.

Specific examples of such an alkylthiocarbamate compound include methylene bis (dibutyldithiocarbamate) and methylenebis [di (2-ethylhexyl) dithiocarbamate].

Examples of the thioterephene compound include a reaction product of phosphorus pentasulfide and pinene, the dialkyl thiodipropionate compound includes, for example, dilauryl thiodipropionate, distearyl thiodipropionate, And mixtures thereof.

The content of the sulfur compound (C) in the lubricating oil composition of the present invention is preferably 0.01% by mass or more, more preferably 0.05% by mass or more, and most preferably 0.1% by mass or less, in terms of the friction characteristics of the obtained lubricating oil composition, More preferably, it is at least% by mass. In addition, the resulting lubricating oil composition is more excellent in separability from the water-soluble cutting fluid, and further improvement of the new friction properties can not be expected even if the lubricating oil composition is contained in a larger amount. The content of the sulfur- By mass or less, more preferably 3% by mass or less, still more preferably 2% by mass or less.

Examples of other known additives include oily agents such as monohydric alcohols or polyhydric alcohols, monobasic acids or polybasic acids, esters of the alcohols with the acids, amines other than the claimed invention 1, and amine compounds such as alkanolamines Phenol compounds such as di-tert-butyl-p-cresol and bisphenol A, and amine-based compounds such as phenyl-α-naphthylamine and N, N'-di (2-naphthyl) Antioxidants such as compounds; Metal deactivators such as benzotriazole and alkyl thiadiazole; Defoaming agents such as silicone oil and fluorosilicone oil; Phosphorus-based additives other than the acidic phosphoric acid ester (such as a phosphoric acid ester, a phosphorous acid ester, and an amine salt of an acidic (phosphoric) acid ester); Oily agents such as carboxylic acids; Rust preventive additives such as alkenyl succinic acid, sorbitan monooleate and the like; pour point depressants such as polymethacrylate; A viscosity index improver such as polymethacrylate, polybutene, polyalkylstyrene, olefin copolymer, styrene-diene copolymer, styrene-maleic anhydride copolymer, and the like.

The lubricating oil composition of the present invention having the above structure is excellent in low friction performance and low temperature storage stability and does not significantly deteriorate the initial low frictional property even when the cutting fluid is mixed, and is also excellent in corrosion resistance. Therefore, it is suitably used for various purposes in the lubricating oil field in which low friction property, low temperature storage stability and corrosion resistance are required. Among them, the effect of the present invention is further exerted when the lubricating oil is used as a lubricating oil for a sliding guide surface (sliding surface) of a machine tool or the like.

Example

Hereinafter, the present invention will be described in more detail based on examples and comparative examples, but the present invention is not limited to the following examples.

[Examples A-1 to A-8, Comparative Examples A-1 to A-4]

In Examples A-1 to A-8 and Comparative Examples A-1 to A-4, lubricating oil compositions described in Tables 1 and 2 were prepared. The components used in the preparation of each composition are as follows. In the present invention, the viscosity index means a viscosity index measured in accordance with JIS K 2283-1993. The content of the saturated hydrocarbon component is determined by the method described in Analytical Chemistry, Vol.44 (6) (1972), pages 915 to 919, "Separation of High-Boiling Petroleum Distillates Using Gradient Elution Through Dual-Packed (Silica Gel-Alumina Gel) Quot; Adsorption Columns ", except that in this method, the saturated hydrocarbon component taken out by the method using n-hexane instead of the n-pentane used for elution of the saturated hydrocarbon component Means the mass percentage of the total sample.

Lubricant base oil:

Base oil 1: solvent refined mineral oil VG68 (viscosity index: 101, sulfur content: 0.51 mass%, saturated hydrocarbon content: 65.6 volume%, kinematic viscosity at 40 占 폚: 68.7 mm2 / s, flash point: 248 占 폚, density at 15 占 폚: g / cm3)

(A) Acidic phosphate ester:

Al: a mixture of mono n-octyl liquid seed phosphate and di-n-octyl liquid seed phosphate (phosphorus content: 11.6% by mass)

A2: A mixture of monooleate solution and monooleate solution (phosphorus content: 6.6% by mass)

A3: Mono n-hexyl liquid seed phosphate (phosphorus content: 17% by mass)

A4: A mixture of mono 2-ethylhexyl liquid seed phosphate and di-2-ethylhexyl liquid seed phosphate (phosphorus content: 12.0% by mass)

(B) alkylamine:

B1: di-2-ethylhexylamine

B2: Diisotridecylamine

B3: 2-ethylhexylamine

B4: oleylamine

(C) Sulfur compound:

C1: polysulfide (sulfur content: 22.0% by mass)

C2: sulfurized oil (sulfur content: 11.4 mass%).

Next, the following tests were carried out on each of the lubricating oil compositions of Examples A-1 to A-8 and Comparative Examples A-1 to A-4.

(Friction Characteristic Evaluation Test)

BRIEF DESCRIPTION OF DRAWINGS FIG. 1 is a schematic diagram showing a friction coefficient measuring system used in a friction characteristic evaluation test. FIG. 1, a table 1 and a movable jig 4 connected to each other via a load cell 5 are arranged on a bed 6. A weight 9 as a substitute for a working tool is provided on the table 1 Respectively. Both the table 1 and the bed 6 are made of cast iron. The movable jig 4 has a bearing portion, which is connected to the A / C servo motor 2 through a feed screw 3. The movable jig 4 can be reciprocated in the axial direction of the feed screw 3 (the direction of the arrow in the figure) by operating the feed screw 3 by the A / C servomotor 2. The computer 7 and the computer 7 and the A / C servomotor 2 are electrically connected to the control panel 8 by the load cell 5 so that the reciprocating motion of the movable jig 4 And the load between the table 1 and the movable jig 4 can be measured.

In this friction coefficient measuring system, after the lubricant composition is dropped on the top surface of the bed 6 and the table weight 9 is selected to adjust the surface pressure between the table 1 and the bed 6 to 200 kPa, The movable jig 4 was reciprocated at a conveyance length of 0.1 mm / min and a conveyance length of 15 mm. The load between the table 1 and the movable jig 4 at this time is measured by the load cell 5 (load meter), and the guide surface (table 1 / bed 6 = cast iron / cast iron ) Was obtained. In addition, the test was conducted after performing the practice operation three times. The friction coefficient of each lubricating oil composition is shown in Tables 1 and 2.

(Test for Evaluating Friction Characteristics when Including Cutting Oil)

500 mL of the lubricating oil composition and 25 mL of a water-soluble cutting fluid (emulsion type cutting fluid, product of Shin-Nippon Sekiyu K.K., a W1 type 1 of JIS K 2241 "cutting oil", dilution ratio of 10 times) were taken in a 1000 mL beaker. In a beaker, the mixture was gently stirred using a magnetic rotor at room temperature for 1 minute. After stirring, the mixture was allowed to stand for 1 hour, and the upper layer was used as a measurement sample. The results of the above friction characteristics evaluation tests are shown in Tables 1 and 2. When the coefficient of friction exceeds 0.110, it is judged that the coefficient of friction is very good if it is within the allowable range, and 0.09 or less if it is outside the allowable range.

(Retention rate of phosphorus when mixed with cutting fluid)

500 mL of the lubricating oil composition and 25 mL of a water-soluble cutting fluid (emulsion type cutting fluid, product of Shin-Nippon Sekiyu K.K., a W1 type 1 of JIS K 2241 "cutting oil", dilution ratio of 10 times) were taken in a 1000 mL beaker. In a beaker, the mixture was gently stirred using a magnetic rotor at room temperature for 1 minute. After the stirring, the mixture was allowed to stand for 1 hour, and the upper layer (oil layer) was used as a measurement sample. Based on JPI test method 5S-38-03 "Lubricating oil-added element test method-Inductively Coupled Plasma Atomic Emission Spectrometry" Minute. (Phosphorus before the test / phosphorus after the test) x 100 was calculated, and the phosphorus residual ratio (%) was determined. The obtained results are shown in Tables 1 and 2.

(Corrosion resistance test when cutting fluid is mixed)

500 mL of the lubricating oil composition and 25 mL of a water-soluble cutting fluid (emulsion type cutting fluid, product of Shin-Nippon Sekiyu K.K., a W1 type 1 of JIS K 2241 "cutting oil", dilution ratio of 10 times) were taken in a 1000 mL beaker. The mixture was gently stirred in a beaker at room temperature for 1 minute using a magnetic rotor. After stirring, the mixture was allowed to stand for 1 hour, used as a measurement sample, taken in a glass beaker at a rate of 200 ml, and dipped in a 7 cm square SPC material (0.2 mm thick and 80 times dulled) . After 20 days, the specimen was rinsed with a solvent, and the appearance was visually observed to evaluate the corrosion resistance by the presence or absence of discoloration at the gas-liquid interface. The evaluation criteria are as follows. The obtained results are shown in Tables 1 and 2.

A: No discoloration

B: tend to slightly discolor

C: Apparently discolored

As is clear from the results shown in Tables 1 and 2, the lubricating oil compositions of Examples A-1 to A-8 had lower friction performance (lower friction coefficient) than the compositions of Comparative Examples A-1 to A-4 , It can be seen that the low friction performance can be maintained even when the cutting oil is mixed and the capability of satisfying the corrosion resistance is also possessed.

[Examples B-1 to B-11]

In Examples B-1 to B-11, lubricating oil compositions having the compositions shown in Tables 3 and 4 are prepared. The components used for preparing each lubricating oil composition are as follows.

Lubricant base oil:

Base oil 1: polyolefin VG32 (viscosity index: 138, sulfur content: less than 1 mass ppm, kinematic viscosity at 40 占 폚: 31.00 mm2 / s, flash point: 246 占 폚, density at 15 占 폚: 0.827 g / Less than 3 ppm)

Base oil 2: wax isomerization base oil VG32 (viscosity index: 154, sulfur content: less than 1 mass ppm, saturated hydrocarbon content: 99.1 mass%, kinematic viscosity at 40 캜: 31.10 mm 2 / s, kinematic viscosity at 100 캜: 6.215 mm 2 / s, Aniline point: 124.9 占 폚, flash point: 258 占 폚, density at 15 占 폚: 0.827 g / cm3, nitrogen content: less than 3 ppm)

Base oil 3: hydrogenated refined base oil VG32 (viscosity index: 135, sulfur content: 0.01 mass%, saturated hydrocarbon content: 97.4 mass%, kinematic viscosity at 40 占 폚: 31.11 mm2 / s, flash point: 246 占 폚, 0.840 g / cm &lt; 3 &gt;, nitrogen content: less than 3 ppm)

Base oil 4: poly-alpha-olefin VG68 (viscosity index: 150, sulfur content: less than 1 mass ppm, kinematic viscosity at 40 DEG C: 69.90 mm2 / s, flash point: 270 DEG C, density at 15 DEG C: 0.842 g / Less than 3 ppm)

Base oil 5: hydrogenated refined base oil VG68 (viscosity index: 110, sulfur content: 0.08 mass%, saturated hydrocarbon content: 76.9 mass%, kinematic viscosity at 40 占 폚: 66.09 mm2 / s, flash point: 258 占 폚, density at 15 占 폚: 0.869 g / cm &lt; 3 &gt;, nitrogen content: 10 ppm)

Base oil 6: poly? -Olefin VG220 (viscosity index: 141, sulfur content: less than 1 ppm, kinematic viscosity at 40 占 폚: 216.0 mm2 / s, flash point: 262 占 폚, density at 15 占 폚: 0.842 g / )

Base oil 7: solvent refined mineral oil VG32 (viscosity index: 102, sulfur content: 0.27% by mass, saturated hydrocarbon fraction: 67.0% by mass, kinematic viscosity at 40 占 폚: 31.54 mm2 / s, flash point: 220 占 폚, density at 15 占 폚: g / cm &lt; 3 &gt;, nitrogen content: 30 ppm)

Base oil 8: Solvent refining base oil VG68 (Viscosity index: 98, sulfur content: 0.62 mass%, saturated hydrocarbon content: 63.9 mass%, kinematic viscosity at 40 占 폚: 68.69 mm2 / s, flash point: 252 占 폚, density at 15 占 폚: 0.885 g / cm &lt; 3 &gt;, nitrogen content: 40 ppm)

Base oil 9: solvent refined mineral oil VG220 (viscosity index: 95, sulfur content: 0.56 mass%, saturated hydrocarbon fraction: 60.1 mass%, kinematic viscosity at 40 占 폚: 215.9 mm2 / s, flash point: 270 占 폚, density at 15 占 폚: 0.894 g / cm &lt; 3 &gt;, nitrogen content: 110 ppm)

The notation of VG32, VG68, and VG220 of the above base oil means a viscosity grade according to JIS K 2001 "Industrial lubricating oil-ISO viscosity classification".

(A) Acidic phosphate ester:

A1: a mixture of mono n-octyl liquid seed phosphate and di-n-octyl liquid seed phosphate (phosphorus content: 11.6% by mass)

A2: A mixture of monooleate solution and monooleate solution (phosphorus content: 6.6% by mass)

(B) alkylamine:

B1: di-2-ethylhexylamine

Other additives:

C1: polysulfide (sulfur content: 22.0% by mass)

Next, the lubricating oil compositions of Examples B-1 to B-11 were subjected to a friction property evaluation test, a friction property evaluation test at the time of incorporating cutting oil, The residual phosphorus ratio at the time of incorporation and the corrosion resistance test at the time of incorporating the cutting fluid were carried out. The obtained results are shown in Tables 3 and 4.

Claims (6)

As a lubricating oil composition,
The composition
Lubricating base oils (lubricating base oils), and
(A) 0.01 to 0.5% by mass of at least one selected from acidic phosphoric acid esters represented by the following general formula (1) or (2), and (B) 0.01 to 2% by mass of an alkylamine represented by the following general formula And / or a reactant,
Wherein the acid value derived from the component (A) is 0.1 to 1.0 mg KOH / g.
Formula 1

(2)

(3)

In the above formulas (1), (2) and (3)
R ¹ and R ² may be the same or different and each is a hydrogen atom or a straight chain alkyl group or a straight chain alkenyl group and at least one of R ¹ and R ² is a straight chain alkyl group or a straight chain alkenyl group having 6 to 12 carbon atoms,
R ³ and R ⁴ may be the same or different and each is a hydrogen atom or a straight chain alkyl group or a straight chain alkenyl group and at least one of R ³ and R ⁴ is a straight chain alkyl group or a straight chain alkenyl group having 13 to 18 carbon atoms,
R ⁵ and R ⁶ may be the same or different and each is a hydrogen atom or a branched alkyl group having 4 to 30 carbon atoms, and at least one of R ⁵ and R ⁶ is a branched chain alkyl group. The lubricating oil composition according to claim 1, wherein the lubricating base oil is a lubricating oil base oil having a viscosity index of 105 or more, a saturated hydrocarbon component of 70 mass% or more, and a sulfur content of 0.2 mass% or less. The lubricating oil composition according to claim 1 or 2, wherein the lubricating oil base oil has a nitrogen content of 10 mass ppm or less, and the lubricating base oil has a flash point of 250 deg. The lubricating oil composition according to claim 1 or 2, further comprising (C) 0.01 to 5% by mass of a sulfur compound based on the total amount of the composition. The lubricating oil composition according to claim 3, further comprising (C) 0.01 to 5% by mass of a sulfur compound based on the total amount of the composition. The lubricating oil composition according to claim 1 or 2, which is used in a machine tool.

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